반응 #936739

반응 방정식

MeOH

5-fluoro-1'-methyl-spiro(2,3-dihydrobenzofuran-3,4'-piperidine)

2-chloroethyl chloroformate

→

title compound

수율 95.1%

5-Fluoro-spiro(2,3-dihydrobenzofuran-3,4'-piperidine)hydrochloride salt

수율 95.1%

용매

1,2-dichloroethane

반응 조건

후처리

1. 1
   기타A white precipitate formed
2. 2
   온도the reaction was refluxed 2 h
3. 3
   온도refluxing
4. 4
   농축The reaction was concentrated to a crude solid, which
5. 5
   기타was triturated with EtOAc (5 mL)
6. 6
   여과filtered

실험 절차

5-fluoro-1'-methyl-spiro(2,3-dihydrobenzofuran-3,4'-piperidine) (1.21 g, 5.48 mmol) in 1,2-dichloroethane (12 mL) at room temp was treated with 2-chloroethyl chloroformate (1 mL, 9 mmol). A white precipitate formed, and the reaction was refluxed 2 h. MeOH (12 mL) was added and refluxing was continued for 2 h. The reaction was concentrated to a crude solid, which was triturated with EtOAc (5 mL) and filtered to yield 1.27 g (95%) of the title compound as a white crystalline solid.

출처